CN112466587A - Dysprosium oxide-coated samarium cobalt permanent magnet material composite powder, and preparation method and system device thereof - Google Patents
Dysprosium oxide-coated samarium cobalt permanent magnet material composite powder, and preparation method and system device thereof Download PDFInfo
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- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 132
- 229910003440 dysprosium oxide Inorganic materials 0.000 title claims abstract description 79
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 96
- 239000012495 reaction gas Substances 0.000 claims abstract description 77
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 67
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000002245 particle Substances 0.000 claims abstract description 66
- 238000002156 mixing Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 62
- 239000012159 carrier gas Substances 0.000 claims description 57
- 230000001681 protective effect Effects 0.000 claims description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 14
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 13
- 239000001307 helium Substances 0.000 claims description 12
- 229910052734 helium Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 4
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- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- BOXVSFHSLKQLNZ-UHFFFAOYSA-K dysprosium(iii) chloride Chemical group Cl[Dy](Cl)Cl BOXVSFHSLKQLNZ-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000009827 uniform distribution Methods 0.000 abstract description 4
- 238000005243 fluidization Methods 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 description 37
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- 229910045601 alloy Inorganic materials 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Abstract
The invention provides dysprosium oxide-coated samarium cobalt permanent magnet material composite powder, a preparation method and a system device thereof, wherein the preparation method comprises the following steps: and mixing the fluidized samarium cobalt particles with a dysprosium source and a reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the dysprosium oxide coated samarium cobalt permanent magnet material composite powder. The method adopts a fluidization process, so that the samarium cobalt powder is fully contacted with a dysprosium source and reaction gas in the fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the powder on a microscopic scale is realized, the uniformity of the permanent magnet on a macroscopic scale is further ensured, and the coercive force of the samarium cobalt permanent magnet material is effectively improved.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and relates to dysprosium oxide-coated samarium cobalt permanent magnet material composite powder, a preparation method and a system device thereof.
Background
The samarium cobalt permanent magnet material has high Curie temperature (TC can reach 923 ℃) and excellent magnetic stability, is the first choice in the high-temperature permanent magnet application field, plays an irreplaceable role in national defense equipment such as electronic communication, electronic interference and countermeasure, accurate guidance and positioning, aerospace and the like, and is one of the hotspots of advanced technical development and strategic competition of countries in the world. In recent years, samarium cobalt permanent magnets have also begun to be used in high power traction motors for subways and high-speed rails. With the rapid development of the industries such as rail transit and the like in China, the demand of samarium cobalt permanent magnet will continuously increase in the future. Thus, samarium cobalt permanent magnets are more and more emphasized by the permanent magnet industry, and the production scale thereof is gradually enlarged in local areas where the permanent magnet industry is concentrated in China.
Samarium cobalt permanent magnet belongs to precipitation hardening permanent magnet material, and the hard magnetism of the samarium cobalt permanent magnet is derived from a unique nano cell structure, and the domain wall movement of a cell-shaped main phase is pinned by a cell wall phase, so that the coercive force is improved. Samarium cobalt permanent magnets have an inhomogeneous reverse magnetization process and therefore squareness is lower than that of permanent magnet materials of the nucleus type, resulting in an actual coercivity of less than 60% of theoretical. Therefore, how to improve the coercive force of the samarium cobalt permanent magnet material becomes a main problem in the field of industrial research.
At present, one effective method for improving the coercivity of a magnet is to dope dysprosium oxide in a permanent magnet material to improve the anisotropy of a magnetic field, so that the coercivity of the magnet can be effectively improved.
CN111161933A discloses a preparation method of a high-coercivity low-temperature-coefficient sintered samarium cobalt permanent magnet, which comprises the following steps: (1) preparing materials (2), smelting an ingot (3), pulverizing (4), mixing materials (5), orientation molding (6), pre-burning, sintering, solid dissolving (7), slicing (8), and preparing a solution: mixing and stirring a dysprosium-containing substance, absolute ethyl alcohol and a dispersing agent to obtain a mixed solution; (9) coating: placing the samarium cobalt alloy thin sheet obtained in the step (7) in the mixed solution obtained in the step (8), soaking and drying; (10) dysprosium infiltration: placing the samarium cobalt alloy thin sheet treated in the step (9) in a vacuum heating furnace, and performing vacuum infiltration; (11) aging treatment: and (5) performing aging treatment on the samarium cobalt alloy sheet treated in the step (10), and cooling to obtain the samarium cobalt permanent magnet.
Therefore, how to design and prepare the high-quality dysprosium oxide coated samarium cobalt permanent magnet material composite powder ensures that components on a microscopic scale are uniformly distributed, and becomes a problem to be solved urgently for improving the coercive force of the samarium cobalt permanent magnet material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the dysprosium oxide coated samarium cobalt permanent magnetic material composite powder, the preparation method and the system device thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of dysprosium oxide-coated samarium cobalt permanent magnet material composite powder, which comprises the following steps:
and mixing the fluidized samarium cobalt particles with a dysprosium source and a reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the dysprosium oxide coated samarium cobalt permanent magnet material composite powder.
The method adopts a fluidization process, so that the samarium cobalt powder is fully contacted with a dysprosium source and reaction gas in the fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the powder on a microscopic scale is realized, the uniformity of the permanent magnet on a macroscopic scale is further ensured, and the coercive force of the samarium cobalt permanent magnet material is effectively improved.
As a preferred embodiment of the present invention, samarium cobalt particles are fluidized in a protective atmosphere to obtain fluidized samarium cobalt particles.
Preferably, the protective gas used in the protective atmosphere comprises at least one of nitrogen, argon or helium or a combination of two groups thereof.
The samarium cobalt particles can be kept in a fluidized state and can isolate oxygen in the environment by reacting in a protective atmosphere, so that the subsequent controllable coating of dysprosium oxide is facilitated.
Preferably, the samarium cobalt particles have a particle size of 0.5 to 100 μm, and may be, for example, 0.5 μm, 1 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or 100 μm, but are not limited to the recited values, and other values not recited within this range are equally applicable.
As a preferred technical solution of the present invention, the mixing manner is: and independently introducing a dysprosium source and reaction gas into the protective atmosphere in which the samarium cobalt particles in the fluidized state are positioned.
Preferably, the mixing temperature is 700 to 800 ℃, for example 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃ or 800, but not limited to the values listed, and other values not listed within the range of values are also applicable.
Preferably, the mixing time is 1min or more, for example 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but is not limited to the values listed, and other values not listed within the range of values are equally applicable.
As a preferred technical scheme of the invention, the dysprosium source is DyCl3。
Preferably, the dysprosium source is preheated and then mixed for reaction.
Preferably, the dysprosium source is preheated to 718-1500 ℃, for example 718 ℃, 720 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃, 1400 ℃, 1450 ℃, or 1500 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the dysprosium source is conveyed into the reaction device through a carrier gas for mixing reaction.
Preferably, the gas velocity of the dysprosium source mixed with the carrier gas is 50-500 mL/min, such as 50mL/min, 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, 350mL/min, 400mL/min, 450mL/min, or 500mL/min, but is not limited to the recited values, and other values not recited in this range are equally applicable.
In a preferred embodiment of the present invention, the reaction gas is steam.
Preferably, the reaction gas is preheated and then mixed for reaction.
Preferably, the reaction gas is preheated to 0 to 100 ℃, for example, 0 ℃, 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the reaction gas is fed into the reaction device through a carrier gas to carry out mixing reaction.
Preferably, the gas velocity of the reaction gas mixed with the carrier gas is 75 to 500mL/min, for example, 75mL/min, 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, 350mL/min, 400mL/min, 450mL/min or 500mL/min, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
The preparation method provided by the invention limits the mixing time and the mixing temperature, and the gas velocity of the dysprosium source and the reaction gas introduced into the fluidized bed reaction device, and realizes the purpose of uniformly depositing dysprosium oxide on the surface of the neodymium iron boron permanent magnet material and the regulation and control of the content of dysprosium oxide by adjusting the process parameters.
As a preferable technical scheme of the invention, the gas-solid separation method comprises gravity settling, centrifugal settling or filtering.
As a preferred technical solution of the present invention, the preparation method comprises:
fluidizing samarium cobalt particles with the particle size of 0.5-100 mu m in a protective atmosphere to obtain fluidized samarium cobalt particles, wherein the protective gas adopted in the protective atmosphere comprises at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
(II) preheating a dysprosium source to 718-1500 ℃, mixing the preheated dysprosium source with carrier gas, and introducing the mixture into a protective atmosphere in which fluidized samarium cobalt particles are located at a gas speed of 50-500 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with carrier gas, and introducing the mixture into the protective atmosphere where the fluidized samarium cobalt particles are located at the gas velocity of 75-500 mL/min, wherein the mixing temperature of the fluidized samarium cobalt particles, the dysprosium source and the reaction gas is 700-800 ℃, and the mixing time is more than or equal to 1 min;
and (III) after the reaction is finished, obtaining the dysprosium oxide coated samarium cobalt permanent magnet material composite powder by gravity settling, centrifugal settling or filtering of the obtained reaction product.
In a second aspect, the invention provides dysprosium oxide-coated samarium cobalt permanent magnet material composite powder prepared by the preparation method in the first aspect, wherein the mass fraction of dysprosium oxide in the dysprosium oxide-coated samarium cobalt permanent magnet material composite powder is 0.1-3.0 wt.%.
The dysprosium oxide-coated samarium cobalt permanent magnet material composite powder provided by the invention is prepared by uniformly coating a dysprosium oxide shell on the surface of samarium cobalt particles by combining a chemical vapor deposition principle and a fluidized bed process technology, and the uniform distribution of microscale ensures the uniformity of macroscale, so as to improve the coercive force of a samarium cobalt permanent magnet material and ensure the component uniformity of a macroscopic permanent magnet motor.
In a third aspect, the invention provides a system device for preparing the dysprosium oxide-coated samarium cobalt permanent magnet material composite powder according to the first aspect, which comprises a fluidized bed reaction device, wherein a protective gas inlet pipe is externally connected to the bottom of the fluidized bed reaction device, a dysprosium source generating device and a reaction gas inlet pipe are respectively and independently and externally connected to the lower part of the reaction device, and a storage bin is externally connected to the upper part of the fluidized bed reaction device.
As a preferable technical scheme, the top of the fluidized bed reaction device is externally connected with a tail gas treatment device.
Preferably, a vaporizing device is arranged on the reaction gas inlet pipe.
Preferably, the fluidized bed reaction device is externally connected with a product collecting device.
The system refers to an equipment system, a system device or a production device.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method adopts a fluidization process, so that the samarium cobalt powder is fully contacted with a dysprosium source and reaction gas in a fluidized bed reaction device, a dynamic basis is provided for subsequent full reaction, the uniform distribution of the powder on a microscopic scale is realized, the uniformity of the permanent magnet on a macroscopic scale is further ensured, and the coercive force of the samarium cobalt permanent magnet material is effectively improved;
(2) the method for preparing the dysprosium oxide-coated samarium cobalt composite powder is simple, uniform in coating layer, controllable in thickness, low in cost and easy for large-scale batch production.
Drawings
Fig. 1 is a schematic structural diagram of a system device for preparing dysprosium oxide-coated samarium cobalt magnetic material composite powder according to an embodiment of the invention;
wherein, 1-a storage bin; 2-a fluidized bed reaction device; a 3-dysprosium source generating device; 4-a vaporization device; 5-a product collection device; 6-tail gas treatment device;
fig. 2 is an SEM image of the dysprosium oxide-coated samarium cobalt composite powder prepared in example 1 of the present invention.
Detailed Description
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "disposed," "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
In a specific embodiment, the invention provides a system device for preparing dysprosium oxide-coated samarium cobalt permanent magnet composite powder, which is shown in fig. 1 and comprises a fluidized bed reaction device 2, wherein a protective gas inlet pipe is externally connected to the bottom of the fluidized bed reaction device 2, the lower part of the reaction device is respectively and independently externally connected with a dysprosium source generating device 3 and a reaction gas inlet pipe, and a vaporizing device 4 is arranged on the reaction gas inlet pipe. The external feed bin 1 in upper portion of fluidized bed reaction unit 2, the external tail gas processing apparatus 6 in top of fluidized bed reaction unit 2, the external product collection device 5 of fluidized bed reaction unit 2.
In another embodiment, the invention provides a preparation method of dysprosium oxide-coated samarium cobalt permanent magnet composite powder, which comprises the following steps:
(1) fluidizing samarium cobalt particles with the particle size of 0.5-100 mu m in a protective atmosphere to obtain fluidized samarium cobalt particles, wherein the protective atmosphere adopts at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
(2) preheating a dysprosium source to 718-1500 ℃, mixing the preheated dysprosium source with carrier gas, and introducing the mixture into a protective atmosphere in which fluidized samarium cobalt particles are located at a gas speed of 50-500 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with carrier gas, and introducing the mixture into the protective atmosphere where the fluidized samarium cobalt particles are located at the gas velocity of 75-500 mL/min, wherein the mixing temperature of the fluidized samarium cobalt particles, the dysprosium source and the reaction gas is 700-800 ℃, and the mixing time is more than or equal to 1 min;
(3) and after the reaction is finished, obtaining the dysprosium oxide coated samarium cobalt permanent magnet material composite powder by carrying out gravity settling, centrifugal settling or filtering on the obtained reaction product.
Example 1
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing nitrogen as shielding gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the shielding atmosphere;
(2) DyCl of dysprosium source3Preheating to 850 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 60 mL/min; preheating the reaction gas to 60 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 80 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 700 ℃ for 30 min;
(3) after the reaction is finished, carrying out gravity settling gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.2 wt.%.
Fig. 2 is an SEM image of the dysprosium oxide-coated samarium cobalt magnetic material composite powder prepared in this example, and it can be seen from fig. 2 that the surface of the samarium cobalt powder is uniformly coated with a layer of dysprosium oxide film.
Example 2
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as protective gas to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 900 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 80 mL/min; preheating the reaction gas to 70 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 120 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 720 ℃ for 90 min;
(3) after the reaction is finished, carrying out centrifugal sedimentation gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.3 wt.%.
Example 3
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing helium gas serving as protective gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 microns to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 1100 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 60 mL/min; preheating the reaction gas to 60 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 100 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 750 ℃ for 60 min;
(3) and after the reaction is finished, carrying out gas-solid separation by filtration to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.5 wt.%.
Example 4
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing nitrogen as shielding gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the shielding atmosphere;
(2) DyCl of dysprosium source3Preheating to 1300 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 120 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 240 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 800 ℃ for 90 min;
(3) after the reaction is finished, carrying out gravity settling gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 2.1 wt.%.
Example 5
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as protective gas to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 900 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 100 mL/min; preheating the reaction gas to 60 deg.C, and feeding it into fluidized bed reactor by carrier gasPlacing the mixture at a speed of 200mL/min for reaction gas and carrier gas; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 770 ℃ for 90 min;
(3) after the reaction is finished, carrying out centrifugal sedimentation gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 1.5 wt.%.
Example 6
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing helium gas serving as protective gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 microns to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 1400 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 160 mL/min; preheating the reaction gas to 80 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 80 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 300 ℃ for 120 min;
(3) and after the reaction is finished, carrying out gas-solid separation by filtration to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 2.2 wt.%.
Example 7
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing nitrogen as shielding gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the shielding atmosphere;
(2) DyCl of dysprosium source3Preheating to 800 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 150 mL/min; preheating the reaction gas to 60 ℃, and then sending the reaction gas into the fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 320 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 730 ℃ for 90 min;
(3) after the reaction is finished, carrying out gravity settling gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 1.4 wt.%.
Example 8
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as protective gas to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 1200 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 80 mL/min; preheating the reaction gas to 50 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 140 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 760 ℃ for 30 min;
(3) after the reaction is finished, carrying out centrifugal sedimentation gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.3 wt.%.
Example 9
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing helium gas serving as protective gas into the fluidized bed reaction device to enable samarium cobalt particles with the particle size of 1-3 microns to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 1000 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 100 mL/min; preheating the reaction gas to 50 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 200 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 800 ℃ for 45 min;
(3) and after the reaction is finished, carrying out gas-solid separation by filtration to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.7 wt.%.
Example 10
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as protective gas to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 718 deg.C, and feeding into fluidized bed reactor 2 with carrier gas, wherein the mixed gas speed of dysprosium source and carrier gas is 50 mL/min; preheating the reaction gas to 10 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 75 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 700 ℃ for 60 min;
(3) after the reaction is finished, carrying out centrifugal sedimentation gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.1 wt.%.
Example 11
The embodiment provides a preparation method of dysprosium oxide-coated samarium cobalt magnetic material composite powder, which is performed in a system device shown in fig. 1, and comprises the following steps:
(1) introducing argon gas into the fluidized bed reaction container as protective gas to enable samarium cobalt particles with the particle size of 1-3 mu m to be in a fluidized state in the protective atmosphere;
(2) DyCl of dysprosium source3Preheating to 1500 ℃, and then sending the mixture into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the dysprosium source and the carrier gas is 500 mL/min; preheating the reaction gas to 100 ℃, and then conveying the reaction gas into a fluidized bed reaction device 2 by carrier gas, wherein the mixed gas speed of the reaction gas and the carrier gas is 500 mL/min; simultaneously introducing a dysprosium source and reaction gas into the fluidized bed reaction device 2, and mixing with fluidized samarium cobalt particles at the mixing temperature of 800 ℃ for 1 min;
(3) after the reaction is finished, carrying out centrifugal sedimentation gas-solid separation to obtain the dysprosium oxide coated samarium cobalt magnetic material composite powder, wherein the content of dysprosium oxide in the dysprosium oxide coated samarium cobalt magnetic material composite powder is 0.3 wt.%.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of dysprosium oxide-coated samarium cobalt permanent magnet material composite powder is characterized by comprising the following steps:
and mixing the fluidized samarium cobalt particles with a dysprosium source and a reaction gas for reaction, and carrying out gas-solid separation on the reaction product to obtain the dysprosium oxide coated samarium cobalt permanent magnet material composite powder.
2. The method of claim 1 in which the samarium cobalt particles are fluidized in a protective atmosphere to provide fluidized samarium cobalt particles;
preferably, the protective gas used in the protective atmosphere comprises at least one of nitrogen, argon or helium or a combination of two groups of nitrogen, argon or helium;
preferably, the samarium cobalt particles have a particle size of 0.5 to 100 μm.
3. The method according to claim 1 or 2, wherein the mixing is performed by: introducing a dysprosium source and a reaction gas into a protective atmosphere in which fluidized samarium cobalt particles are positioned respectively and independently;
preferably, the mixing temperature is 700-800 ℃;
preferably, the mixing time is more than or equal to 1 min.
4. The process according to any one of claims 1 to 3, wherein the source of dysprosium is DyCl3；
Preferably, the dysprosium source is preheated and then mixed for reaction;
preferably, the dysprosium source is preheated to 718-1500 ℃;
preferably, the dysprosium source is conveyed into the reaction device through a carrier gas for mixing reaction;
preferably, the gas velocity after the dysprosium source and the carrier gas are mixed is 50-500 mL/min.
5. The production method according to any one of claims 1 to 4, wherein the reaction gas is water vapor;
preferably, the reaction gas is preheated and then is mixed for reaction;
preferably, the reaction gas is preheated to 0-100 ℃;
preferably, the reaction gas is sent into the reaction device through a carrier gas to carry out mixing reaction;
preferably, the gas velocity after the reaction gas and the carrier gas are mixed is 75-500 mL/min.
6. The process according to any one of claims 1 to 5, wherein the gas-solid separation comprises gravity settling, centrifugal settling or filtration.
7. The method according to any one of claims 1 to 6, wherein the method comprises:
fluidizing samarium cobalt particles with the particle size of 0.5-100 mu m in a protective atmosphere to obtain fluidized samarium cobalt particles, wherein the protective gas adopted in the protective atmosphere comprises at least one of nitrogen, argon or helium or the combination of two groups of nitrogen, argon or helium;
(II) preheating a dysprosium source to 718-1500 ℃, mixing the preheated dysprosium source with carrier gas, and introducing the mixture into a protective atmosphere in which fluidized samarium cobalt particles are located at a gas speed of 50-500 mL/min; meanwhile, preheating the reaction gas to 0-100 ℃, mixing the preheated reaction gas with carrier gas, and introducing the mixture into the protective atmosphere where the fluidized samarium cobalt particles are located at the gas velocity of 75-500 mL/min, wherein the mixing temperature of the fluidized samarium cobalt particles, the dysprosium source and the reaction gas is 700-800 ℃, and the mixing time is more than or equal to 1 min;
and (III) after the reaction is finished, obtaining the dysprosium oxide coated samarium cobalt permanent magnet material composite powder by gravity settling, centrifugal settling or filtering of the obtained reaction product.
8. The dysprosium oxide-coated samarium cobalt permanent magnet material composite powder prepared by the preparation method of any one of claims 1-7 is characterized in that the mass fraction of dysprosium oxide in the dysprosium oxide-coated samarium cobalt permanent magnet material composite powder is 0.1-3.0 wt.%.
9. A system device for preparing the dysprosium oxide-coated samarium cobalt permanent magnet material composite powder according to claim 8, comprising a fluidized bed reaction device, wherein the bottom of the fluidized bed reaction device is externally connected with a protective gas inlet pipe, the lower part of the reaction device is respectively and independently externally connected with a dysprosium source generating device and a reaction gas inlet pipe, and the upper part of the fluidized bed reaction device is externally connected with a storage bin.
10. The system device according to claim 9, wherein the top of the fluidized bed reactor is externally connected with a tail gas treatment device;
preferably, a vaporizing device is arranged on the reaction gas inlet pipe;
preferably, the fluidized bed reaction device is externally connected with a product collecting device.
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| US20140271323A1 (en) * | 2013-03-15 | 2014-09-18 | GM Global Technology Operations LLC | Manufacturing nd-fe-b magnets using hot pressing with reduced dysprosium or terbium |
| CN109647293A (en) * | 2018-11-07 | 2019-04-19 | 中国科学院过程工程研究所 | A kind of system and method for anode material for lithium-ion batteries metal oxide coating modification |
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